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CN113130111A - Hole-filling printing slurry for HTCC and preparation method thereof - Google Patents

Hole-filling printing slurry for HTCC and preparation method thereof Download PDF

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Publication number
CN113130111A
CN113130111A CN201911395628.5A CN201911395628A CN113130111A CN 113130111 A CN113130111 A CN 113130111A CN 201911395628 A CN201911395628 A CN 201911395628A CN 113130111 A CN113130111 A CN 113130111A
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parts
powder
htcc
pore
filling printing
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刘永良
潘亚蕊
赵鑫
卢红霞
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Zhengzhou Dengfeng Power Galaxy Technology Co ltd
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Zhengzhou Dengfeng Power Galaxy Technology Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/14—Conductive material dispersed in non-conductive inorganic material
    • H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
    • H01L23/488—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of soldered or bonded constructions
    • H01L23/498—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers
    • H01L23/49866—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers characterised by the materials
    • H01L23/49883—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers characterised by the materials the conductive materials containing organic materials or pastes, e.g. for thick films

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  • Physics & Mathematics (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Computer Hardware Design (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Inorganic Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Manufacturing & Machinery (AREA)
  • Printing Elements For Providing Electric Connections Between Printed Circuits (AREA)
  • Conductive Materials (AREA)

Abstract

The invention belongs to the technical field of semiconductor manufacturing, and particularly relates to a pore-filling printing slurry for HTCC and a preparation method thereof. The pore-filling printing slurry is prepared from the following raw materials in parts by weight: 75-85 parts of metal powder, 9-12 parts of inorganic additive and 8-10 parts of organic carrier, wherein the metal powder is tungsten powder or mixed powder consisting of tungsten powder and molybdenum powder, and the inorganic additive is prepared from aluminum oxide: silica (7-10): (1-3) parts by weight of an organic carrier, wherein the organic carrier comprises the following components in parts by weight: slurry auxiliary agent: binder (6-10): (0.03-0.06): (0.5 to 2) by weight. The invention realizes good smoothness after slurry hole filling and sintering through selection of various raw material types and proportions, does not influence the proceeding of downstream processing procedures, and has high yield.

Description

Hole-filling printing slurry for HTCC and preparation method thereof
Technical Field
The invention belongs to the technical field of semiconductor manufacturing, and particularly relates to a pore-filling printing slurry for HTCC and a preparation method thereof.
Background
The functional ceramic material provides important support for modern electronic information technology, and has wide application in the fields of energy, communication, household appliances, automobiles and the like. The co-fired multilayer ceramic substrate can satisfy various requirements of integrated circuits by embedding passive elements such as signal lines, micro-wires and the like into the substrate by using a thick film technology, and is receiving more and more attention. The co-fired multilayer ceramic substrate can be divided into a high temperature co-fired multilayer ceramic (HTCC) substrate and a low temperature co-fired multilayer ceramic (LTCC) substrate, wherein the alumina ceramic substrate becomes an ideal ceramic substrate material due to the characteristics of high thermal conductivity, high electrical insulation strength, low dielectric constant and the like.
Taking an alumina ceramic packaging base as an example, the process mainly comprises the steps of printing filling hole printing slurry on a ceramic green ceramic chip through screen printing, and laminating, sintering, electroplating and other processes of a plurality of layers of green ceramic chips to realize the process of ceramic metallization. Taking the structure of a typical ceramic package base as an example, the ceramic package base can be simply understood as a three-layer structure: lower base plate, upper base plate, metal frame. The lower substrate (as shown in fig. 1) is printed with conductive circuit metal paste, and the upper substrate (as shown in fig. 2) is also printed with metal paste with special shape, so as to match with the brazing metal frame, and the structure of the metal frame is shown in fig. 3; the key for realizing the conduction of the lower substrate and the upper substrate is to fill the hole and print slurry, and the finished ceramic packaging base is shown in fig. 4. The general production process can be summarized as follows: mixing, ball milling → defoaming → casting green ceramic chip → blanking → punching → hole filling, printing conductive circuit → laminated hot isostatic pressing → discharging glue → sintering → primary nickel plating → stamping sealing metal frame → brazing → secondary nickel electroplating → gold plating → splitting → detection → packaging → warehousing.
The hole-filling printing slurry is a necessary medium for realizing the conduction of the multilayer ceramic substrate, and is a powerful means for realizing low resistance, high precision and high reliability of electronic component products. Pore-filling printing pastes generally consist of three main components: functional powder phases, glass binder phases and organic vehicles, generally require pore-filling printing pastes that have good electrical conductivity, good high temperature stability, and are able to comply with component miniaturization requirements. In the prior art, chinese patent application CN103361531A discloses a high-temperature co-fired ceramic slurry, which comprises, by weight, 17 to 61.7 wt% of tungsten powder, 4 to 48.5 wt% of molybdenum powder, 0 to 20 wt% of an inorganic additive, and 18 wt% of an organic carrier, and the resistance temperature coefficient of the slurry is adjusted by adjusting the proportion of tungsten and molybdenum in the slurry, so as to meet the requirements of different electronic components.
At present, the hole filling process mostly adopts a screen printing hole filling mode, a schematic diagram of the hole filling process is shown in fig. 5, each plate comprises a bushing 4, a green ceramic sheet 3, air permeable paper 2 and a porous ceramic table 1 from top to bottom in sequence, wherein the bushing is made of stainless steel. During filling, when the scraper 5 moves to the right (as shown by the arrow at the upper part of fig. 5), and the pressure on the scraper 5 is applied to the bushing to press the slurry 6 into the holes of the bushing, the porous ceramic table 1 is vacuumed from the bottom of the green ceramic sheet 3 through the air permeable paper 2 to help the slurry 6 to fill the whole micropores.
The existing hole filling printing slurry only focuses on the conductivity (such as temperature coefficient of resistance, conductivity), stability and the like of the slurry, but in the practical application process, even if the indexes meet the use requirements, the phenomenon of base air leakage often occurs in the subsequent processing processes of lamination, braze welding and the like, and the metal frame is easy to shift during framing, so that the yield is influenced.
Disclosure of Invention
The invention aims to provide a hole-filling printing paste for HTCC (high temperature co-fired ceramic), which is used for solving the problems that the existing high-temperature co-fired ceramic paste is easy to leak gas after being made into a ceramic base and a metal frame is deviated during framing.
Another object of the present invention is to provide a method for preparing a hole-filling printing paste for HTCC, which solves the problems of easy occurrence of air leakage, metal frame shift during framing, and microcracks due to inconsistent shrinkage degree after sintering metal paste and ceramic substrate after manufacturing a ceramic base from a paste obtained by the conventional method for preparing a hole-filling printing paste.
In order to achieve the above object, the specific technical solution of the pore-filling printing paste for HTCC of the present invention is:
the pore-filling printing slurry for the HTCC comprises the following raw materials in parts by weight: 75-85 parts of metal powder, 9-12 parts of inorganic additive and 8-10 parts of organic carrier, wherein the metal powder is tungsten powder or mixed powder consisting of tungsten powder and molybdenum powder, and the inorganic additive is prepared from aluminum oxide: silica (7-10): (1-3) parts by weight of an organic carrier, wherein the organic carrier comprises the following components in parts by weight: slurry auxiliary agent: binder (6-10): (0.03-0.06): (0.5 to 2) by weight.
HTCC is with porefilling printing thick liquids at the porefilling in-process, the porefilling plumpness that fills in the thick liquids in the ceramic green chip hole direct influence green ceramic chip, and if the degree of thick liquids inflation or shrink behind the sintering does not match with ceramic base member, can finally influence the planarization of sintering back ceramic substrate (aluminium oxide ceramic substrate), protrusion or sunken degree are too big promptly, and then the metal frame braze welding connection effect of the electric connection between the direct influence ceramic substrate or ceramic substrate and back process, thereby cause ceramic base gas leakage.
According to the invention, by adjusting the proportion of the metal powder, the inorganic additive and the organic carrier in the raw materials of the hole-filling printing slurry for HTCC, and selecting the type and the proportion of the inorganic additive and the organic carrier, the filling degree of the hole-filling printing slurry poured into the holes of the ceramic green ceramic chip after screen printing is proper under the premise that hole-filling jigs (screen printing plates and scrapers) are not changed, and meanwhile, the hole-filling printing slurry and the HTCC substrate are well matched after sintering, so that the effect of no protrusion or recess (within an acceptable range) is achieved, and the implementation of downstream processing procedures is not influenced. The metal powder, the inorganic additive and the organic carrier are compounded in proportion to form slurry with appropriate viscosity, generally speaking, the Brookfield HB (Brookfield HB) viscosity range is 1RPM 700-1500kcPs, and the components meet the requirements of hole filling and smoothness after sintering, so that the yield is high.
The inorganic additive taking alumina as a main component can generate a compound with good bonding strength with alumina ceramic in the sintering process, so that the bonding between particles in the slurry is realized. The slurry assistant in the organic vehicle generally plays a role in increasing the fluidity and uniformity of the slurry, enhancing the flexibility of the organic vehicle, and the like.
Further, the metal powder is selected to be pure tungsten powder, and the metal powder comprises the following raw materials in parts by weight: 80-85 parts of tungsten powder, 8-9 parts of inorganic additive and 9-10 parts of organic carrier, and the tungsten powder, the inorganic additive and the organic carrier are compounded, so that the slurry can meet the performance of smoothness after hole filling and sintering.
The metal powder can also be mixed powder consisting of 42-67 parts by weight of tungsten powder and 13-36 parts by weight of molybdenum powder. The density of tungsten is 19.2g/cm due to different specific gravity of tungsten and molybdenum3The density of the molybdenum is 10.2g/cm3The organic carriers in the slurry with the same quality bear different weights, the printing plumpness of the slurry with different tungsten and molybdenum contents is different, the sheet resistance is also different, the sheet resistance can reflect the electric conduction performance of the material to a certain degree, and the contents of tungsten and molybdenum in the slurry are adjusted according to the requirements of different electronic elements on the smoothness and sheet resistance of the slurry filled hole and the sintered substrate, so that the requirements of low resistance, high precision and high reliability of electronic components are met. Moreover, the thermal expansion coefficients of the tungsten and the molybdenum are relatively close to that of the high-temperature ceramic, and product cracks cannot occur due to different expansion coefficients after sintering.
The solvent needs to select substances with moderate volatility, different solvents have optimal flash point gradient matching use effects, the dry and wet degree of the printed slurry directly influences the production efficiency of the product, and the solvent is prepared from terpineol and tributyl citrate in parts by weight (5-8): (1-1.8).
The sizing agent auxiliary agent comprises a plasticizer, a thixotropic agent and a flatting agent, and the weight ratio of the plasticizer to the thixotropic agent to the flatting agent is (0.01-0.02): (0.01-0.03): (0.01-0.02), and the performance of the three components is optimal after the three components are matched with each other in the proportion. The thixotropic agent is also called as an anti-sagging agent and plays roles of shear thinning and thickening in a standing state under the stress condition; the leveling agent can enable the slurry to have certain flowability and enable the slurry to have the characteristics of smoothness, uniformity and the like; the plasticizer is used for enhancing the flexibility of the organic carrier, and the thixotropic agent, the flatting agent and the plasticizer supplement each other in the screen printing process, so that the optimal printing effect is ensured.
The binder needs to be selected from substances which have good wettability to a substrate material, certain bonding strength, quick drying and less residue after binder removal and sintering, and the binder can be selected from ethyl cellulose or polyvinyl butyral.
The preparation method of the pore-filling printing slurry for HTCC comprises the following specific technical scheme:
a preparation method of hole-filling printing slurry for HTCC comprises the following steps:
(1) mixing metal powder and inorganic additive, wet grinding, drying, pulverizing and sieving to obtain mixed powder;
(2) and uniformly mixing the plasticizer, the thixotropic agent and the flatting agent to obtain an organic carrier, and mixing and grinding the organic carrier and the mixed powder to obtain the composite material.
The preparation method of the hole-filling printing slurry for HTCC adopts a wet milling mode to ball mill and mix tungsten powder, molybdenum powder and inorganic additives, the wet milling can ball-mill conglomerates into fine particles, the ball milling time is short, slurry with uniform and consistent components can be obtained, powder particles in the slurry are mainly round particles rather than flaky particles, the hole-filling printing slurry for subsequent manufacture has better fluidity and obtains larger stacking density, and therefore, the effects of low resistance and high conduction are obtained, and the defects that the dry milling has high energy consumption, the powder is too fine (micron-sized), the ceramic ball/cylinder lining wall is adhered, the discharging is difficult, the operating conditions are poor, fine dust flies, the environmental pollution is serious, the health of operating workers is seriously damaged and the like are avoided.
The preparation method of the invention realizes the large-scale production with simple production process, industrialization and low cost of the hole-filling printing slurry, and simultaneously realizes the application of the hole-filling printing slurry to different electronic components and can meet the requirements of low resistance, high precision and high reliability.
In order to make the particle size suitable, the time for wet grinding is 96-120 h.
The particle size of the metal powder in the raw material is mainly selected according to the particle size of the powder in the ceramic substrate and the thickness of the substrate. Generally, the particle size of the metal powder is 0.5 to 3 μm.
The particle size of the inorganic additive in the raw material should not be larger than that of the metal powder, wherein the particle size of the alumina is generally 1-2 μm.
In order to obtain mixed powder with proper granularity, a screen mesh used for sieving is 200-250 meshes.
Drawings
FIG. 1 is a bottom substrate of a conventional ceramic package base printed with metal paste;
FIG. 2 is a top substrate printed with metal paste in a conventional ceramic package base;
FIG. 3 is a metal frame of a conventional ceramic package base;
FIG. 4 is a prior art ceramic package base assembly;
FIG. 5 is a schematic diagram illustrating a hole filling process in a conventional screen printing process;
FIG. 6 is a schematic illustration of hole-filling with a hole-filling printing paste, post-sintering bulging less than 5 μm using the HTCC of the present invention;
FIG. 7 is a schematic illustration of hole-filling with a hole-filling printing paste using the HTCC of the present invention with a post-sintering dishing of less than 5 μm;
wherein:
in FIG. 5, 1-porous ceramic stage; 2-breathable paper; 3-green ceramic chip; 4-in a bushing; 5-a scraper; 6-slurry;
in fig. 6 and 7, the hatched portions represent the ceramic substrates, and the black filled portions represent the hole-filling printing paste for HTCC.
Detailed Description
The following examples are provided to further illustrate the practice of the invention.
First, a concrete example of the hole-filling printing paste for HTCC of the invention
Example 1
The pore-filling printing paste for the HTCC of the embodiment is prepared from the following raw materials in parts by weight: 83 parts of tungsten powder; 0 part of molybdenum powder; 9 parts of inorganic additive, wherein 7 parts of alumina and 2 parts of silicon dioxide are contained; the organic carrier comprises 8 parts of organic carrier, wherein 5.57 parts of terpineol, 1.2 parts of tributyl citrate, 0.03 part of a sizing agent assistant, 1.2 parts of binder ethyl cellulose, 0.01 part of plasticizer, 0.01 part of thixotropic agent and 0.01 part of flatting agent in the sizing agent assistant, wherein the plasticizer is dibutyl phthalate, the thixotropic agent is hydrogenated castor oil, and the flatting agent is lecithin.
Example 2
The pore-filling printing paste for the HTCC of the embodiment is prepared from the following raw materials in parts by weight: 67 parts of tungsten powder; 13 parts of molybdenum powder; 10 parts of inorganic additive, wherein 8 parts of alumina and 2 parts of silicon dioxide are contained; the organic carrier comprises 10 parts of organic carrier, wherein the terpineol comprises 6.95 parts of terpineol, 1.5 parts of tributyl citrate, 0.05 part of a slurry auxiliary agent, 1.5 parts of adhesive polyvinyl butyral, 0.01 part of plasticizer, 0.025 part of thixotropic agent and 0.015 part of flatting agent, the plasticizer is dibutyl phthalate, the thixotropic agent is hydrogenated castor oil, and the flatting agent is lecithin.
Example 3
The pore-filling printing paste for the HTCC of the embodiment is prepared from the following raw materials in parts by weight: 42 parts of tungsten powder; 36 parts of molybdenum powder; 10 parts of inorganic additive, wherein 8 parts of alumina and 2 parts of silicon dioxide are contained; 12 parts of organic carrier, wherein 8.45 parts of terpineol and 1.7 parts of tributyl citrate are contained; 0.05 part of a sizing agent additive; 1.8 parts of binder ethyl cellulose, 0.01 part of plasticizer in the sizing agent, 0.025 part of thixotropic agent and 0.015 part of flatting agent, wherein the plasticizer is dibutyl phthalate, the thixotropic agent is hydrogenated castor oil, and the flatting agent is lecithin.
Second, specific examples of the method for preparing a via-filling printing paste for HTCC according to the present invention
Example 4
A method for preparing a via-filling printing paste for HTCC according to this embodiment describes a process for preparing a via-filling printing paste for HTCC according to embodiment 1, and specifically includes the following steps:
(1) putting tungsten powder, alumina powder and silicon dioxide into a ball milling tank, mixing and ball milling for 96h by taking absolute ethyl alcohol as ball milling liquid and alumina balls as ball milling medium, filtering out the alumina balls by a 100-mesh screen, and drying in an oven at 80 ℃ for 12 h;
(2) crushing the dried mixture, and then sieving the crushed mixture through a 250-mesh sieve to obtain mixed powder;
(3) uniformly mixing the plasticizer, the thixotropic agent and the leveling agent to obtain an organic carrier, adding the organic carrier into the mixed powder, premixing by a high-speed shearing machine, and rolling by a three-roll grinding machine to obtain the hole-filling printing slurry for the HTCC.
Example 5
A method for preparing a via-filling printing paste for HTCC according to this embodiment describes a process for preparing a via-filling printing paste for HTCC according to embodiment 2, and specifically includes the following steps:
(1) putting tungsten powder, molybdenum powder, alumina powder and silicon dioxide into a ball milling tank, mixing and ball milling for 96h by taking absolute ethyl alcohol as ball milling liquid and alumina balls as ball milling media, filtering the alumina balls by a 100-mesh screen, and drying in an oven at 80 ℃ for 12 h;
(2) crushing the dried mixture, and then sieving the crushed mixture through a 200-mesh sieve to obtain mixed powder;
(3) uniformly mixing the plasticizer, the thixotropic agent and the leveling agent to obtain an organic carrier, adding the organic carrier into the mixed powder, premixing by a high-speed shearing machine, and rolling by a three-roll grinding machine to obtain the hole-filling printing slurry for the HTCC.
Example 6
A method for preparing a via-filling printing paste for HTCC according to this embodiment describes a process for preparing a via-filling printing paste for HTCC according to embodiment 3, and specifically includes the following steps:
(1) putting tungsten powder, molybdenum powder, alumina powder and silicon dioxide into a ball milling tank, mixing and ball milling for 120h by taking absolute ethyl alcohol as ball milling liquid and alumina balls as ball milling media, filtering the alumina balls by a 100-mesh screen, and drying in an oven at 80 ℃ for 12 h;
(2) crushing the dried mixture, and then sieving the crushed mixture through a 200-mesh sieve to obtain mixed powder;
(3) uniformly mixing the plasticizer, the thixotropic agent and the leveling agent to obtain an organic carrier, adding the organic carrier into the mixed powder, premixing by a high-speed shearing machine, and rolling by a three-roll grinding machine to obtain the hole-filling printing slurry for the HTCC.
Third, comparative example
Comparative example 1
The pore-filling printing paste for the HTCC of the comparative example comprises the following raw materials in parts by weight: 89 parts of tungsten powder; 0 part of molybdenum powder; 6 parts of inorganic additive, wherein 5 parts of alumina and 1 part of silicon dioxide are contained; the organic carrier comprises 5 parts of organic carrier, wherein 3.475 parts of terpineol, 0.75 part of tributyl citrate, 0.025 part of a sizing agent assistant, 0.75 part of binder ethyl cellulose, 0.005 part of plasticizer, 0.01 part of thixotropic agent and 0.01 part of flatting agent in the sizing agent assistant, wherein the plasticizer is dibutyl phthalate, the thixotropic agent is hydrogenated castor oil, and the flatting agent is lecithin.
Comparative example 2
The pore-filling printing paste for HTCC of this comparative example had the same raw material composition as the pore-filling printing paste for HTCC of example 1 except that: the powder is not subjected to ball milling treatment in the preparation process, and the mixed raw materials are directly dried and rolled.
Fourth, example of experiment
The hole filling printing slurry for HTCC of the embodiments 1 to 3 and the comparative examples 1 and 2 is subjected to hole filling and sintering by adopting a screen printing technology, and the hole filling process adopts a method introduced in the background technology. The protrusion or indentation of the slurry after sintering is schematically shown in fig. 6 and 7, and the performance data of the HTCC is shown in table 1.
TABLE 1 Performance data of pore-filling printing pastes for HTCC of examples 1 to 3 after pore-filling and sintering
Figure BDA0002346227330000061
Figure BDA0002346227330000071
In the production process, after the green ceramic chips are subjected to hole filling, lamination and sintering, the problem of poor slurry smoothness is easily caused by the influence of slurry fullness and the mismatching of slurry expansion performance and a substrate in the sintering process, even a substrate crack is generated, and the situation that more defective products are generated is easily caused. From the above results, it can be seen that the composition of the hole-filling printing paste has a great influence on the flatness and yield of the product. By using the same hole-filling printing method, the hole-filling printing slurry formula for the HTCC can obviously improve the smoothness of the slurry, can control the protrusion or the recess within an acceptable range, and obviously improves the yield. When the solid content in the slurry is higher, as in comparative example 1, when the viscosity 1RPM is greater than 2000kcPs, the process progress is not directly influenced by the stencil hole filling printing, the protrusion of the filled hole after sintering is greater than 20 μm, and the yield is greatly reduced and is less than 50%. In addition, if the raw materials are not subjected to ball milling treatment, as in comparative example 2, the prepared pore-filling slurry is not uniform, the problem of mismatching caused by inconsistent shrinkage degree (inconsistent thermal expansion performance) of the metal slurry and the ceramic substrate after sintering is easily caused in the later sintering process due to nonuniform or non-compact slurry in the pores, and the yield is greatly reduced by the generated microcracks, which is less than 50%.
The invention realizes the smoothness of the sintered ceramic substrate and the metal slurry filled in the ceramic substrate by mainly adjusting the proportion of the metal powder, the inorganic additive and the organic carrier. For the ceramic base, after ceramic metallization, the sheet resistance value is less than 1 omega, the basic requirement can be met, the protrusion is within an acceptable range within 20 micrometers, if the hole filling printing slurry is excessively protruded after sintering, the carrying of a metal frame in the subsequent brazing process can be influenced, and the yield is greatly reduced. As can be seen from the comparison of the performance data in table 1, the pore-filling printing paste for HTCC obtained by using the raw material composition and the compounding ratio in example 3 has good flatness after pore filling and sintering, and high yield.

Claims (10)

1. The pore-filling printing paste for the HTCC is characterized by comprising the following raw materials in parts by weight: 75-85 parts of metal powder, 9-12 parts of inorganic additive and 8-10 parts of organic carrier, wherein the metal powder is tungsten powder or mixed powder consisting of tungsten powder and molybdenum powder, and the inorganic additive is prepared from aluminum oxide: silica (7-10): (1-3) parts by weight of an organic carrier, wherein the organic carrier comprises the following components in parts by weight: slurry auxiliary agent: binder (6-10): (0.03-0.06): (0.5 to 2) by weight.
2. The pore-filling printing paste for the HTCC according to claim 1, wherein the metal powder is tungsten powder, and the metal powder comprises the following raw materials in parts by weight: 80-85 parts of tungsten powder, 8-9 parts of inorganic additive and 9-10 parts of organic carrier.
3. The pore-filling printing paste for HTCC according to claim 1, wherein said metal powder is a mixed powder of tungsten powder and molybdenum powder, wherein the weight part of tungsten powder is 42-67 parts, and the weight part of molybdenum powder is 13-36 parts.
4. The pore-filling printing paste for HTCC according to any one of claims 1 to 3, wherein said solvent comprises terpineol and tributyl citrate in a weight ratio of (5-8): (1-1.8).
5. The pore-filling printing paste for HTCC according to any one of claims 1 to 3, wherein the paste auxiliaries are a plasticizer, a thixotropic agent and a leveling agent, and the weight ratio of the plasticizer to the thixotropic agent to the leveling agent is (0.01-0.02): (0.01-0.03): (0.01-0.02).
6. The pore-filling printing paste for HTCC according to any one of claims 1 to 3, wherein said binder is ethyl cellulose or polyvinyl butyral.
7. The method of preparing a pore-filling printing paste for HTCC according to claim 1, comprising the steps of:
(1) mixing metal powder and inorganic additive, wet grinding, drying, pulverizing and sieving to obtain mixed powder;
(2) and uniformly mixing the plasticizer, the thixotropic agent and the flatting agent to obtain an organic carrier, and mixing and grinding the organic carrier and the mixed powder to obtain the composite material.
8. The method for preparing a pore-filling printing paste for HTCC according to claim 7, wherein said wet-milling time is 96 to 120 hours.
9. The method for preparing a pore-filling printing paste for HTCC according to claim 7, wherein said metal powder has a particle size of 0.5 to 3 μm.
10. The method for preparing a hole-filling printing paste for HTCC according to any one of claims 7 to 9, wherein a screen used for said sieving is 200 to 250 mesh.
CN201911395628.5A 2019-12-30 2019-12-30 Hole-filling printing slurry for HTCC and preparation method thereof Pending CN113130111A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115073148A (en) * 2022-07-21 2022-09-20 瓷金科技(河南)有限公司 Ceramic packaging base and preparation method thereof
CN115424761A (en) * 2022-08-18 2022-12-02 大连海外华昇电子科技有限公司 Tungsten slurry for HTCC substrate and preparation method thereof
CN116646108A (en) * 2023-04-27 2023-08-25 成都宏科电子科技有限公司 Organic carrier, pore-filling slurry and preparation method

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CN115073148A (en) * 2022-07-21 2022-09-20 瓷金科技(河南)有限公司 Ceramic packaging base and preparation method thereof
CN115073148B (en) * 2022-07-21 2023-08-08 瓷金科技(河南)有限公司 Ceramic packaging base and preparation method thereof
CN115424761A (en) * 2022-08-18 2022-12-02 大连海外华昇电子科技有限公司 Tungsten slurry for HTCC substrate and preparation method thereof
CN116646108A (en) * 2023-04-27 2023-08-25 成都宏科电子科技有限公司 Organic carrier, pore-filling slurry and preparation method

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Application publication date: 20210716